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Sodium Carbonate → 2-Cyano-4'-methylbiphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Chlorobenzonitrile | HCID 13391 | — |
| 反応物 | Tolylboronic acid | HCID 79799 | — |
| 反応物 | Sodium 3,3',3''-phosphinetriyltribenzenesulfonate hydrate | HCID 53487040 | — |
| 触媒 | palladium(II) acetate | HCID 167845 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | P-Xylene | HCID 7809 | — |
| 生成物 | 2-Cyano-4'-methylbiphenyl | HCID 145512 | 89.8% |
反応手順
15 g of 2-chlorobenzonitrile, 14.8 g of p-tolueneboronic acid and 28.9 g of sodium carbonate in 50 ml of p-xylene, 40 ml of glycol and 10 ml of water were heated to 120° C. At 80° C., a mixture of 24.7 mg of palladium acetate and 0.55 ml of TPPTS/H2O solution (0.6 molar) in 2.5 ml of DMSO was added. After the reaction was complete, the phases were separated. The aqueous phase was washed with 50 ml of toluene. The combined organic phases were washed with 20 ml of water and subsequently dried over sodium sulfate. Crystallization from n-heptane gave 18.9 g of 2-cyano-4'-methylbiphenyl.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06140265 |
| 出典データセット | uspto-grants-2000_10 |
| ORD ID | ord-16377a5c3720489b9dcb0d577904c77b |
| 出典メモ | uspto-grants-2000_10 |